Summary of the invention
In view of this, in order to address the above problem, it is the transformer oil preparation method of raw material with the vegetables oil that the present invention provides a kind of.
The objective of the invention is to realize like this, is the transformer oil preparation method of raw material with the vegetables oil, comprises the steps:
1) vegetable oil material is carried out the alkali neutralization;
2) in the alkali with after vegetable oil material carry out underpressure distillation;
3) vegetable oil material after the underpressure distillation is carried out hydrogenation;
4) vegetable oil material after the hydrogenation is carried out dark refining: dark purified purpose is to remove the trace copper of enzymatic oxidation effect with Hydrocerol A.Add the Hydrocerol A that accounts for vegetable oil material weight 0.3-1.0%, underpressure distillation 1-2 hour, pressure 20-50mmHg, temperature 80-90 ℃ in the vegetable oil material after hydrogenation; Add the bentonite that accounts for vegetable oil material weight 0.1-0.3%, underpressure distillation 1-2 hour, pressure 20-50mmHg, temperature 80-90 ℃ again;
5) vegetable oil material after the dark refining is carried out underpressure distillation once more;
6) add additive in the vegetable oil material after underpressure distillation once more.
Further, said vegetables oil is one or more in rapeseed oil, VT 18, sweet oil, sunflower seed oil, peanut oil, camellia seed oil and the Oleum Gossypii semen;
Further, also comprise the step that vegetable oil material is decoloured in the step 1);
Further, said step 1) comprises the steps:
11) in 5~10min, the NaOH solution that accounts for vegetable oil material weight 1%~4% of adding and oily equality of temperature carries out the alkali neutralization; Behind the 30min, carry out vegetable oil material is washed with the zero(ppm) water of equality of temperature, then standing demix; Separation of fatty acids and sodium hydroxide neutralized reaction product sodium soap leave standstill more than the 30min then, with vacuum distillation apparatus oil sample are distilled 30min again; Stop heating, remove vacuum;
12) in alkali with after vegetable oil material add the discoloring agent account for vegetable oil material weight 2.0~5.0%; Decompression and heating, residual voltage 20~50mmHg in the container, 90~95 ℃ of oil temperature, bleaching time 20~30min after decolouring finishes, is cooled to 70 ℃, removes vacuum;
13) repeating step 11) and 12), until the vegetable oil material clear, and acid number≤0.03mgKOHg
-1
Further, said step 2) specifically comprising the steps: to keep the container residual voltage is 20~50mmHg, and 95 ℃ of oil temperature are distilled and removed moisture, elimination impurity in 2-4 hour;
Further, said step 3) specifically comprises the steps: to add the catalyzer that accounts for vegetable oil material weight 0.4%~0.5%, under sealing, nitrogen environment, heats up by 5~10 ℃/min; Keep 180~200 ℃ of temperature, pressure 0.15~0.2MPa, stir speed (S.S.) 300~700rmin
-1, in vegetable oil material, feed hydrogen, hydrogenation 130min~180min;
Further, it is 20~50mmHg that said step 5) specifically comprises the steps: to keep the container residual voltage, and the oil temperature is distilled and removed moisture suction filtration then, impurity such as elimination catalyzer in 2-4 hour at 95 ℃;
Further; The additive that adds in the said step 6) comprises inhibitor; It is 0.2%~0.5% of vegetable oil material weight that said inhibitor adds weight, and said inhibitor is selected from DBPC 2,6 ditertiary butyl p cresol, 4; 4-methylene-bis (2,6 di t butyl phenol), certain herbaceous plants with big flowers base phenyl alpha-naphthylamine (korenyl alpha-naphthylamine), tertiarybutylhydroquinone, tea-polyphenol and Rosmarinus officinalis;
Further; Said additive also comprises metal passivator; It is 0.1%~0.5% of vegetable oil material weight that said metal passivator adds weight, and said metal passivator is one or more in Methylbenzotriazole verivate, liquid triazole verivate or the triazole tetrahydrobenzene.
Compared with prior art, the present invention has following advantage:
(1) transformer insulation oil of present method production is obtained through refining by vegetables oil, does not contain Toxic matter, can not damage environment and human body, and biological degradation fast and up hill and dale, be a kind of environment-friendly type insulated liquid;
(2) transformer insulation oil of present method production is a kind of flame retardant resistance transformer insulation oil, and its flash-point and burning-point all are higher than 300 ℃, can be applied to the place that high fire resistance requires, and the risk of presence of fire and blast is all far below traditional transformer oil;
(3) this transformer oil has good physics and chemistry and dielectric properties, and acid number is lower than 0.03mg KOH/g, and condensation point is lower than-18 ℃, and frequency breakdown voltage surpasses 70kV, and 90 ℃ of Jie's damage value tg δ are lower than 0.0075, and volume specific resistance is higher than 7 * 1010 Ω m, and specific inductivity is 2.93.The performance constant can reach or be higher than the standard as insulating liquid in the electricinstallation; Other performance index also meet the standard GB 2536-90 of mineral transformer oil fully.
Other advantages of the present invention, target; To in specification sheets subsequently, set forth to a certain extent with characteristic; And to a certain extent,, perhaps can from practice of the present invention, obtain instruction based on being conspicuous to those skilled in the art to investigating of hereinafter.Target of the present invention and other advantages can be passed through following specification sheets, claims, and the structure that is particularly pointed out in the accompanying drawing realizes and obtains.
Embodiment
Below will carry out detailed description to the preferred embodiments of the present invention.
Embodiment 1:
1) selecting the transgenic rapeseed oil of high oleic acid content and camellia seed oil for use is raw material, and vegetable oil material is carried out alkali neutralization and decolouring, specifically comprises the steps:
11) in 10min, the NaOH solution that accounts for vegetable oil material weight 1% of adding and oily equality of temperature carries out the alkali neutralization; Behind the 30min, carry out vegetable oil material is washed with the zero(ppm) water of equality of temperature, then standing demix; Separation of fatty acids and sodium hydroxide neutralized reaction product sodium soap leave standstill more than the 30min then, with vacuum distillation apparatus oil sample are distilled 30min again; Stop heating, remove vacuum;
12) in alkali with after vegetable oil material add the discoloring agent account for vegetable oil material weight 2.0%; Decompression and heating, residual voltage 35mmHg in the container, 90 ℃ of oil temperature, bleaching time 20min after decolouring finishes, is cooled to 70 ℃, removes vacuum;
13) repeating step 11) and 12), until the vegetable oil material clear, and acid number≤0.03mgKOHg
-1
2) in the alkali with after vegetable oil material carry out underpressure distillation: keeping the container residual voltage is 20mmHg, 95 ℃ of oil temperature, stirring velocity is 25rmin
-1, distilling and removed moisture in 3 hours, suction filtration is gone out impurity such as discoloring agent;
3) vegetable oil material after the underpressure distillation is carried out hydrogenation: add the catalyzer that accounts for vegetable oil material weight 0.5%, under sealing, nitrogen environment, heat up by 10 ℃/min; Keep 185 ℃ of temperature, pressure 0.15MPa, stir speed (S.S.) 300rmin
-1, in vegetable oil material, feed hydrogen, hydrogenation 130min;
4) vegetable oil material after the hydrogenation is carried out dark refining: add the Hydrocerol A that accounts for vegetable oil material weight 0.5%, underpressure distillation 1.5 hours, pressure 20mmHg, 85 ℃ of temperature in the vegetable oil material after hydrogenation; Add the bentonite that accounts for vegetable oil material weight 0.3% again, underpressure distillation 1.5 hours, pressure 20mmHg, 90 ℃ of temperature, stirring velocity are 25rmin
-1
5) vegetable oil material after the dark refining is carried out underpressure distillation once more: keeping the container residual voltage is 20mmHg, and the oil temperature is distilled and removed moisture suction filtration then, impurity such as elimination catalyzer in 3 hours at 95 ℃;
6) add oil in the vegetable oil material after underpressure distillation once more and weigh 0.3% inhibitor 4,4-methylene-bis (2,6 di t butyl phenol) and oil weigh 0.1% metal passivator IRGAMET 39, then ultra-sonic oscillation to transparent clarification.
Embodiment 2
1) selecting sweet oil for use is raw material, and vegetable oil material is carried out alkali neutralization and decolouring, specifically comprises the steps:
11) in 5min, the NaOH solution that accounts for vegetable oil material weight 4% of adding and oily equality of temperature carries out the alkali neutralization; Behind the 30min, carry out vegetable oil material is washed with the zero(ppm) water of equality of temperature, then standing demix; Separation of fatty acids and sodium hydroxide neutralized reaction product sodium soap leave standstill more than the 30min then, with vacuum distillation apparatus oil sample are distilled 30min again; Stop heating, remove vacuum;
12) in alkali with after vegetable oil material add the discoloring agent account for vegetable oil material weight 5%; Decompression and heating, residual voltage 50mmHg in the container, 95 ℃ of oil temperature, bleaching time 30min after decolouring finishes, is cooled to 70 ℃, removes vacuum;
13) repeating step 11) and 12), until the vegetable oil material clear, and acid number≤0.03mgKOHg
-1
2) in the alkali with after vegetable oil material carry out underpressure distillation: keeping the container residual voltage is 35mmHg, 95 ℃ of oil temperature, stirring velocity is 25rmin
-1, distilling and removed moisture in 2 hours, suction filtration is gone out impurity such as discoloring agent;
3) vegetable oil material after the underpressure distillation is carried out hydrogenation: add the catalyzer that accounts for vegetable oil material weight 0.4%, under sealing, nitrogen environment, heat up by 5 ℃/min; Keep 185 ℃ of temperature, pressure 0.15MPa, stir speed (S.S.) 700rmin
-1, in vegetable oil material, feed hydrogen, hydrogenation 150min;
4) vegetable oil material after the hydrogenation is carried out dark refining: add the Hydrocerol A that accounts for vegetable oil material weight 0.5%, underpressure distillation 1.5 hours, pressure 20mmHg, 80 ℃ of temperature in the vegetable oil material after hydrogenation; Add the bentonite that accounts for vegetable oil material weight 0.3% again, underpressure distillation 1 hour, pressure 20mmHg, 80 ℃ of temperature, stirring velocity are 25rmin
-1
5) vegetable oil material after the dark refining is carried out underpressure distillation once more: keeping the container residual voltage is 40mmHg, and the oil temperature is distilled and removed moisture suction filtration then, impurity such as elimination catalyzer in 3 hours at 95 ℃;
6) adding oil in the vegetable oil material after underpressure distillation once more weighs 0.5% inhibitor DBPC 2,6 ditertiary butyl p cresol and oil and weighs 0.4% metal passivator IRGAMET 39, ultra-sonic oscillation to transparent clarification then.
Embodiment 3:
1) selecting VT 18 for use is raw material, and vegetable oil material is carried out alkali neutralization and decolouring, specifically comprises the steps:
11) in 8min, the NaOH solution that accounts for vegetable oil material weight 3% of adding and oily equality of temperature carries out the alkali neutralization; Behind the 30min, carry out vegetable oil material is washed with the zero(ppm) water of equality of temperature, then standing demix; Separation of fatty acids and sodium hydroxide neutralized reaction product sodium soap leave standstill more than the 30min then, with vacuum distillation apparatus oil sample are distilled 30min again; Stop heating, remove vacuum;
12) in alkali with after vegetable oil material add the discoloring agent account for vegetable oil material weight 3.5%; Decompression and heating, residual voltage 20mmHg in the container, 93 ℃ of oil temperature, bleaching time 25min after decolouring finishes, is cooled to 70 ℃, removes vacuum;
13) repeating step 11) and 12), until the vegetable oil material clear, and acid number≤0.03mgKOHg
-1
2) in the alkali with after vegetable oil material carry out underpressure distillation: keeping the container residual voltage is 50mmHg, 95 ℃ of oil temperature, stirring velocity is 25rmin
-1, distilling and removed moisture in 4 hours, suction filtration is gone out impurity such as discoloring agent;
3) vegetable oil material after the underpressure distillation is carried out hydrogenation: add the catalyzer that accounts for vegetable oil material weight 0.4%, under sealing, nitrogen environment, heat up by 8 ℃/min; Keep 185 ℃ of temperature, pressure 0.15MPa, stir speed (S.S.) 300rmin
-1, in vegetable oil material, feed hydrogen, hydrogenation 180min;
4) vegetable oil material after the hydrogenation is carried out dark refining: add the Hydrocerol A that accounts for vegetable oil material weight 0.3%, underpressure distillation 1.5 hours, pressure 50mmHg, 85 ℃ of temperature in the vegetable oil material after hydrogenation; Add the bentonite that accounts for vegetable oil material weight 0.1% again, underpressure distillation 2 hours, pressure 35mmHg, 85 ℃ of temperature, stirring velocity are 25rmin
-1
5) vegetable oil material after the dark refining is carried out underpressure distillation once more: keeping the container residual voltage is 50mmHg, and the oil temperature is distilled and removed moisture suction filtration then, impurity such as elimination catalyzer in 3 hours at 95 ℃;
6) adding oil in the vegetable oil material after underpressure distillation once more weighs 0.5% certain herbaceous plants with big flowers base phenyl alpha-naphthylamine (korenyl alpha-naphthylamine) and oil and weighs 0.2% metal passivator IRGAMET 39, ultra-sonic oscillation to transparent clarification then.
Embodiment 4
1) selecting Oleum Gossypii semen for use is raw material, and vegetable oil material is carried out alkali neutralization and decolouring, specifically comprises the steps:
11) in 10min, the NaOH solution that accounts for vegetable oil material weight 1% of adding and oily equality of temperature carries out the alkali neutralization; Behind the 30min, carry out vegetable oil material is washed with the zero(ppm) water of equality of temperature, then standing demix; Separation of fatty acids and sodium hydroxide neutralized reaction product sodium soap leave standstill more than the 30min then, with vacuum distillation apparatus oil sample are distilled 30min again; Stop heating, remove vacuum;
12) in alkali with after vegetable oil material add the discoloring agent account for vegetable oil material weight 2%; Decompression and heating, residual voltage 20mmHg in the container, 95 ℃ of oil temperature, bleaching time 30min after decolouring finishes, is cooled to 70 ℃, removes vacuum;
13) repeating step 11) and 12), until the vegetable oil material clear, and acid number≤0.03mgKOHg
-1
2) in the alkali with after vegetable oil material carry out underpressure distillation: keeping the container residual voltage is 22mmHg, 95 ℃ of oil temperature, stirring velocity is 25rmin
-1, distilling and removed moisture in 3 hours, suction filtration is gone out impurity such as discoloring agent;
3) vegetable oil material after the underpressure distillation is carried out hydrogenation: add the catalyzer that accounts for vegetable oil material weight 0.45%, under sealing, nitrogen environment, heat up by 7 ℃/min; Keep 185 ℃ of temperature, pressure 0.15MPa, stir speed (S.S.) 500rmin
-1, in vegetable oil material, feed hydrogen, hydrogenation 180min;
4) vegetable oil material after the hydrogenation is carried out dark refining: add the Hydrocerol A that accounts for vegetable oil material weight 0.5%, underpressure distillation 2 hours, pressure 25mmHg, 90 ℃ of temperature in the vegetable oil material after hydrogenation; Add the bentonite that accounts for vegetable oil material weight 0.2% again, underpressure distillation 1.5 hours, pressure 50mmHg, 90 ℃ of temperature, stirring velocity are 25rmin
-1
5) vegetable oil material after the dark refining is carried out underpressure distillation once more: keeping the container residual voltage is 50mmHg, and the oil temperature is distilled and removed moisture suction filtration then, impurity such as elimination catalyzer in 3 hours at 95 ℃;
6) adding oil in the vegetable oil material after underpressure distillation once more weighs 0.5% inhibitor tertiarybutylhydroquinone and oil and weighs 0.5% metal passivator IRGAMET 39, ultra-sonic oscillation to transparent clarification then.
Among the foregoing description 1-4, discoloring agent can adopt atlapulgite, Calcium Chloride Powder Anhydrous, molecular sieve, the composite discoloring agent of gac etc., best, select the atlapulgite of following method preparation for use: get 2molL
-1Sulfuric acid 50ml, bentonite 30g puts into 90 ℃ heating bath and heats, stirring velocity 20~30rmin after the mixing
-1, continuously stirring 4.5 hours, repeatedly washing makes PH=4~5, and centrifugal separation is separated out atlapulgite, dries 2 hours down for 110 ℃, and oven dry is ground to 200 mesh sieves; Catalyzer can be selected for use in the step 3): copper-nickel binary catalyst or metallic nickel catalyzer.
In the present invention; Choose the oxidation inhibitor, the metal passivator that are complementary with the plant type transformer oil; Can further improve the antioxidative stabilizer of plant type transformer oil, the more important thing is the insatiable hunger degree that has suitably improved the vegetables oil molecule in addition, fundamentally improve the resistance of oxidation of oil.
The leading indicator of the vegetable insulating oil of the present invention's preparation is following:
Parameter |
Vegetables oil |
Transformer oil (GB 2536-90) |
Outward appearance |
Faint yellow, transparent |
Transparent, inclusion-free |
Flash-point/℃ |
325 |
≥135 |
Acid number/mgKOHg
-1 |
0.02 |
≤0.03 |
Water soluble acid/pH |
5.6 |
- |
Frequency breakdown voltage/kV |
73.0 |
≥35 |
Be situated between and decrease tg δ (90 ℃)/% |
0.75 |
≤0.5 |
Volume specific resistance (90 ℃)/Ω m |
7×10
10 |
≥6×10
10 |
Relative permittivity (90 ℃) |
2.93 |
- |
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.